JP2004012339A - Metal specimen quick collection sampler and method for quick sampling using the same - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a sampler for collecting a specimen immediately provided for a component analysis and to provide a method for quickly sampling the same. <P>SOLUTION: The metal specimen quick collecting sampler for quickly collecting a metal specimen from a molten metal includes (a) a quenching material having at least one flat surface for quickly solidifying the molten metal provided as a core of at least one sampler, (b) a space partitioning plate of a material which repels the molten metal mounted oppositely to the flat surface, and (c) a specimen forming space for forming the metal sample by quickly solidifying the molten metal in the space between the flat surface and the space partitioning plate. <P>COPYRIGHT: (C)2004,JPO

Description

[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention provides a metal sample used for rapid discrimination of metal components in order to perform process control quickly and accurately in a metal refining process, particularly a metal sample suitable for component analysis by a spark emission spectrometer. And a sampling method using the sampler.
[0002]
[Prior art]
In the metal refining process, a metal sample is collected by a sampler, the components are analyzed by an analytical instrument, and the components of the metal are controlled or adjusted. This management and adjustment requires quick and accurate, but in order to perform the above management and adjustment quickly and accurately, first, it is necessary to quickly collect a metal sample and quickly provide it for analysis.
[0003]
Conventionally, a cylindrical sampler (a sampler in which a molten metal 2 is pumped in a container 1) whose basic structure is shown in FIG. 1 is frequently used for collecting a metal sample. However, since the collected metal sample is cylindrical, It takes a long time of 400 seconds or more to prepare a sample of a predetermined shape (for example, flake shape) suitable for analysis from the sample.
[0004]
Conventionally, spark emission spectroscopy has been frequently used for analysis because it can be analyzed quickly, and the analysis itself does not take much time. As far as the cylindrical sampler is used, considerable time is required as described above.
[0005]
Therefore, in order to shorten the time from sampling to analysis, various samplers for quickly collecting a sample have been proposed.
[0006]
For example, Japanese Unexamined Utility Model Publication No. 6-74964 proposes a probe for collecting a molten metal sample in which a sample collecting container and a pin sample collecting container are attached to the end of a paper tube, and a disk sample and a pin sample are simultaneously sampled. Japanese Patent Application Laid-Open No. Hei 9-21795 discloses that a small block sample collection chamber is provided in addition to a sample collection chamber, and a sample to be used for emission spectroscopy or X-ray fluorescence analysis and a sample to be used for fuel gas analysis are simultaneously collected. Metal sampling devices have been proposed.
[0007]
However, the sample collected by these samplers is not as large as the sample collected by the cylindrical sampler, but the sample diameter is large and the sample thickness is large. It also takes a considerable amount of time before analysis is performed, and the sampler is inferior in obtaining the analysis results quickly.
[0008]
Furthermore, in the sampler, central component segregation occurs due to a difference in solidification rate at the time of cooling, a metal structure is enlarged with a delay in the solidification rate, and inclusions such as cementite are precipitated, and emission spectroscopy is performed. There is a problem in both analysis time and analysis accuracy that abnormal light emission occurs during analysis and analysis accuracy is impaired.
[0009]
However, in the metal refining process in recent years, it is essential that component management and adjustment be performed promptly and accurately. Therefore, it is strongly desired to minimize the time from sampling to obtaining analysis results. ing.
[0010]
[Problems to be solved by the invention]
An object of the present invention is to provide a sampler for collecting a sample which can be immediately subjected to component analysis and a sampling method for rapidly collecting a sample using the sampler in order to meet the above-mentioned demand.
[0011]
[Means for Solving the Problems]
The present inventors have investigated the causes of the delay in analysis time and the deterioration in analysis accuracy in metal samples collected by a conventional sampler. As a result, it was found that the delay of the analysis time and the deterioration of the analysis accuracy were caused by the thick sample for analysis.
[0012]
That is, since the molten metal starts to solidify from the moment it comes into contact with the mold wall, in a conventional sampler (for example, a cylindrical sampler), the molten metal is sufficiently introduced into the interior of the sample collection container to obtain a uniform component. In order to prepare a sample, the thickness of the sample had to be increased, but it was found that this was a cause of a delay in analysis time and a deterioration in analysis accuracy.
[0013]
The present inventor initially thought that, in order to shorten the time of sampling, if the molten metal is pumped into a flake and coagulated at the same time, a flaky sample that can be directly used for analysis could be obtained. Based on the idea described above, the structure of the sampler was examined, and as shown in FIG. 2, a thick-bottom type sampler having a dish-shaped concave portion 4 for accommodating the molten metal 2 on the upper portion of the quenching body 3 was prototyped.
[0014]
In this thick-bottom sampler, the molten metal 2 contained in the dish-shaped recess 4 is rapidly cooled by the quenching body 3 and solidified, so that the time required for sampling is greatly reduced, which is suitable for speeding up sampling. However, on the other hand, if the thickness of the collected metal sample is not constant and the sample thickness is too thin, it becomes difficult to hold the sample during polishing for analysis, and safety measures to prevent scattering of the metal sample Some points to be improved have emerged, such as the need for
[0015]
However, since the effect of shortening the sampling time by using the quenching body 3 is extremely large, the present inventor has proposed a structure of a sampler capable of collecting a metal sample by reducing the sample thickness to the minimum while maintaining this effect. Was further studied.
[0016]
As a result, the present inventor has determined that a plate made of a material that is resistant to thermal shock, has excellent heat resistance, has a small amount of metal impurities, and repels a molten metal (hereinafter, sometimes referred to as a “heat-resistant repellent plate”) is a quenched body. When a flat space (hereinafter sometimes referred to as a “flat space”) is defined between the heat-resistant plate and the plane of the quenching body, the heat-resistant repellent plate is provided. The molten metal quickly and smoothly penetrates into the flat space, and the plane of the quenching body rapidly solidifies the intruding molten metal, making it possible to extremely quickly form a thin metal sample with good surface properties. I found that I can create it.
[0017]
The present inventor has conducted experiments using plates of various materials as a heat-resistant repelling plate. As a result, in addition to a quartz glass plate, a glass plate and a boron nitride plate can be used. It has been found that a plate coated with a high-temperature lubricating / release material (for example, ceramic powder such as boron nitride, silica, alumina, zirconia, silicon carbide, etc.) on the surface layer can be used. According to the experimental results of the inventor, when the molten metal is molten steel, a quartz glass plate is suitable.
[0018]
In addition, the present inventor has considered in the past that in a cylindrical sampler, a mold (container) and a solidified metal were often welded to each other, and it took time to remove a metal sample, which hindered the speed of analysis. In the present invention, conversely, the molten metal is deliberately welded to the plane (wall) of the quenched body together with the rapid solidification to form a metal sample, and the metal sample is left as it is (without peeling off the plane (wall) of the quenched body). The idea was that analysis should be performed using the smooth sample surface on the heat-resistant repelling plate side as the analysis surface for analysis, and the sample separation / removal process that was conventionally considered to be an inevitable process in the sampling process was performed. By omitting, we succeeded in significantly reducing the overall sampling time.
[0019]
Furthermore, conventionally, in the case of many samplings, only one sample is collected in the sampling container, which causes the inconvenience that if the sample is defective, the sample must be re-sampled. At the same time, the inventor has further studied means for resolving the above-mentioned inconvenience and for resolving the factors which hinder the rapid analysis.
[0020]
As a result, if a flat space is defined on the left and right sides with the heat-resistant repelling plate interposed between the planes of the two quenching bodies, two samples (one is a copy sample) are made simultaneously by one immersion of the sampler. It is only necessary to select one of the most suitable samples for analysis, and if one of the samples is defective, it is not necessary to resample it, eliminating the above inconvenience and speeding up the analysis. The idea was that the factors that hindered could be eliminated.
[0021]
The present invention has been made based on the above findings and ideas, and the gist is as follows.
[0022]
(1) In a sampler that collects a metal sample from molten metal,
(A) providing at least one quenched body having at least one plane for rapidly solidifying a molten metal as a core part of a sampler;
(B) facing the plane, mounting a space partition plate made of a material that repels molten metal;
(C) The space between the plane and the space partition plate is a sample forming space in which the molten metal is rapidly solidified to form a metal sample.
A sampler for rapidly collecting metal samples.
[0023]
(2) The metal sample rapid sampling sampler according to the above (1), wherein the quenching body is made of a material having a high heat removal ability.
[0024]
(3) The material according to (2), wherein the material having a high heat removal ability is a material composed of one or more of iron, steel, aluminum, copper, and stainless steel. Metal sample rapid sampling sampler.
[0025]
(4) The metal sample rapid as described in any one of (1) to (3) above, wherein the space partition plate is a plate made of a material having excellent thermal shock resistance and heat resistance and having a small amount of metal impurities. Collection sampler.
[0026]
(5) The sampler according to (4), wherein the plate made of a material having a small amount of metal impurities is a quartz glass plate.
[0027]
(6) The sampler according to any one of (1) to (5), wherein the thickness of the sample forming space is 0.5 to 20 mm.
[0028]
(7) The sampler according to any one of (1) to (6), wherein the sample forming space has a gas vent hole.
[0029]
(8) The metal sample quick as described in any one of (1) to (7) above, wherein the quenching bodies are combined so that the planes face each other with a space partition plate interposed therebetween to form a core portion. Collection sampler.
[0030]
(9) In a sampling method of immersing a sampler in a molten metal and collecting a metal sample to be analyzed,
(A) immersing the metal sample rapid sampling sampler according to any of (1) to (8) above in a molten metal;
(B) quenching and solidifying the molten metal to form a metal sample in a sample forming space between the plane where the molten metal of the quenched body is rapidly solidified and the space dividing plate;
(C) peeling the space partition plate after pulling up the sampler and cooling,
A rapid sampling method characterized by the above-mentioned.
[0031]
(10) In a sampling method for immersing a sampler in a molten metal and collecting a metal sample to be analyzed,
(A) immersing the metal sample rapid sampling sampler according to any of (1) to (8) above in a molten metal;
(B) quenching and solidifying the molten metal to form a metal sample in a sample forming space between the plane where the molten metal of the quenched body is rapidly solidified and the space dividing plate;
(C) After the sampler is pulled up and cooled, the space partition plate is peeled off,
(D) subjecting the metal sample to polishing and analysis while being welded to the flat surface of the quenched body,
A rapid sampling method characterized by the above-mentioned.
[0032]
BEST MODE FOR CARRYING OUT THE INVENTION
The present invention will be described in detail.
[0033]
The metal sample rapid sampling sampler according to the present invention,
A quenched body having at least one plane for rapidly solidifying the molten metal is provided as a core portion of at least one sampler. (A) The quenched body having at least one plane for rapidly solidifying the molten metal is opposed to the plane of the quenched body, Attach a space partition plate made of material that repels molten metal,
(B) the space between the plane of the quenching body and the space partition plate is a flat sample forming space in which the intruded molten metal is quenched and solidified to form a metal sample;
That is the basic idea.
[0034]
FIG. 3 shows an embodiment of the core section 12 of the sampler for rapidly collecting metal samples. As shown in FIG. 3, a spacer 6 is formed on the upper side surface of the quenching body 3 opposite to the mounting surface of the support rod 9 so that a space partition plate 5 made of a material repelling molten metal covers one side surface of the quenching body 3. Are sandwiched between them, and are attached to the side walls of the depression 8 formed on the upper surface of the quenching body 3 and the clip 7 that sandwiches the spacer 6 and the space partition plate 5.
[0035]
As described above, a flat sample forming space (hereinafter, referred to as “sample forming space”) in which the molten metal 2 enters and solidifies to form the metal sample 11 is defined on the lower side surface of the quenching body 3.
[0036]
In this case, the sample formation space may be open in both the width direction and the lower part, may be closed in the width direction and opened in the lower part, or may be closed in the lower part and opened in the width direction. Any one may be selected in consideration of the type and characteristics of the molten metal.
[0037]
The thickness of the sample formation space is adjusted by adjusting the thickness of the spacer 6 or reducing the thickness of the lower side surface as shown in FIG. In addition, the height of the sample forming space can be appropriately adjusted, but the thickness and / or height of the sample forming space is appropriately set in consideration of the type and characteristics of the molten metal.
[0038]
The quenching body 3 is made of a material having a high heat removal capability in order to rapidly and solidify the molten metal accurately. As a material having a high heat removal ability, a material composed of one or more of iron, steel, aluminum, copper, and stainless steel can be used. According to the experimental results of the present inventors, when the molten metal is molten steel, iron or steel is preferable.
[0039]
In the present invention, a plate made of a material that repels molten metal is used as the space partition plate 5. The space partition plate 5 is desirably a plate made of a material having excellent thermal shock resistance and heat resistance and a small amount of metal impurities, in addition to a material that repels molten metal.
[0040]
According to the experimental results of the present inventor, a quartz glass plate, a glass plate, a boron nitride plate is used as a space partition plate, and a high-temperature lubricating / release material (for example, boron nitride, silica, A plate coated with ceramic powder (alumina, zirconia, silicon carbide, etc.) can be used.
[0041]
The space partition plate may be made of an appropriate material depending on the type and characteristics of the molten metal. When the molten metal is molten steel, a quartz glass plate is preferred.
[0042]
The material of the spacer 6 may be any material that is fire-resistant and heat-resistant and has a function as a spacer. However, the same material as that of the space partition plate 5 is economical and preferable.
[0043]
Further, since the core portion 12 is repeatedly immersed in the molten metal, it is preferable to cover all or a part of the side surface of the quenched body 3 with the ceramic lubricant 10 to extend the life.
[0044]
Further, for example, if a gas vent hole is provided between the quenching body 3 and the spacer 6 or through the spacer 6, the molten metal can be quickly and smoothly introduced into the sample forming space. Preferably, the holes are provided in some manner.
[0045]
Then, in the present invention, the sample forming space and the space partition plate 3 work together in an important manner, and a metal sample that can be immediately used for analysis can be prepared. This operation will be described.
[0046]
When the core portion 12 of the sampler is rapidly immersed in the molten metal, the molten metal enters the sample forming space. However, on the opposite surface of the quenching body 3, there is a space partition plate 5 made of a material that repels the molten metal. The molten metal quickly and smoothly penetrates into the sample forming space without being solidified near the insertion port of the sample forming space.
[0047]
After the molten metal fills the sample forming space, the molten metal is quenched by the quenching body 3 and solidified to form the metal sample 11.
[0048]
The metal sample 11 is handled while being welded to the plane (side wall) of the quenching body 3 and subjected to polishing and analysis. In the analysis, the sample surface formed on the side of the space partition plate 5 is used. , Used as an analysis surface.
[0049]
As described above, the thickness and / or height of the sample forming space is appropriately set in consideration of the type and characteristics of the molten metal, and the thickness and / or height are determined in the metal sample in the thickness direction. Is important in obtaining a uniform solidified structure in each of the height direction and the width direction.
[0050]
The optimum range of the thickness and / or height varies depending on the type and characteristics of the molten metal, but in the case of molten steel, the thickness is preferably 0.5 to 20 mm. In this case, the height may be an appropriate height.
[0051]
If the thickness is less than 0.5 mm, it is difficult for the molten steel to enter the sample forming space, while if it exceeds 20 mm, the solidified structure becomes uneven or the molten steel falls off during the lifting. And a smooth surface cannot be obtained.
[0052]
The more preferable thickness of the sample forming space is 1 to 5 mm, and about 2 mm is even more preferable in terms of the speed of sampling and the smoothness of the metal sample surface.
[0053]
Here, FIG. 4 shows an overall embodiment of the metal sample rapid sampling sampler according to the present invention. In the sampler shown in FIG. 4, the support rod 9 of the core part 12 is inserted into a holding support rod 15 protected by a refractory ceramic cylinder 13, and the entire core part 12 is inserted into a slag mixing prevention paper cylinder 14. Protected.
[0054]
When the sampler for rapidly collecting a metal sample is immersed in the molten metal for several seconds, the molten metal is quickly and smoothly solidified without solidifying at the insertion port of the sample forming space due to the presence of the space partition plate 5 having a property of repelling the molten metal. It enters the inside of the forming space, is quenched by the quenching body 3 and solidifies to form the metal sample 11.
[0055]
Thereafter, the sampler is pulled up and water-cooled, and then an impact is applied to the space partition plate 5 and the clip 7 to separate the space partition plate 3 from the quenching body 3 to form a smooth surface (formed on the side of the space partition plate 3). Surface) can be obtained.
[0056]
In the rapid sampling method of the present invention, the metal sample 11 is handled in a state of being welded to the quenching body 3, and after polishing the smooth surface to make it even smoother, for example, the sample is supplied to an emission spectrometer, To analyze.
[0057]
Further, according to the rapid sampling method of the present invention, the metal sample 11 is handled in a state of being welded to the quenching body 3, so that the sample removing step which has been conventionally considered to be an inevitable step can be omitted. And the overall sampling time can be significantly reduced.
[0058]
Further, in the present invention, as shown in FIG. 5, the two core portions can be combined symmetrically about the space partition plate 5 to form a “two-piece core portion”. With such a configuration, two pieces of the same metal sample 11 can be obtained at the same time while being welded to the cooling body 3, so that either one can be selected as an optimum analysis target sample, and one metal sample 11 can be selected. Even if is poor in solidification structure, one of the metal samples can be used, and it is not necessary to take the metal sample again, and the speed of polishing and analysis is not hindered.
[0059]
【Example】
Next, examples of the present invention will be described, but the present invention is not limited to the conditions employed in the examples.
[0060]
(Example)
A sampler having a core portion having the structure shown in FIG. 3 is manufactured using a steel quenching body having a length of 30 mm × a width of 30 mm × a height of 50 mm, and the rapid sampling method of the present invention (the method of the present invention) and the conventional sampling method ( In the conventional method), molten steel was sampled and the analysis time and analysis accuracy were compared.
[0061]
Regarding the analysis time, it was confirmed that the conventional method required about 120 seconds to take out the sample, while the method of the present invention could reduce the thickness of the sample to about 2 mm and took out the sample after about 20 seconds.
[0062]
Regarding the analysis accuracy, the amount of Ti was analyzed by emission spectroscopy and compared. FIG. 6 shows the result. As shown in this figure, since the Ti content in both samples obtained by the method of the present invention and the conventional method has a corresponding relationship, the sample obtained by the method of the present invention is different from the sample obtained by the conventional method in terms of analytical accuracy. It can be seen that the sample can be replaced with a sample collected by the conventional method.
[0063]
As described above, according to the sampling method of the present invention, an appropriate sample that can be immediately provided for emission spectroscopy can be quickly collected.
[0064]
【The invention's effect】
According to the present invention, when the metal sample rapid sampling sampler is pulled up, the molten metal is rapidly solidified inside the sample forming space to form the metal sample, and furthermore, the metal sample is still welded to the quenched body. Since the sample is handled, the step of taking out the sample can be omitted, the time from cooling up to cooling and subjecting to polishing can be greatly reduced, and the component management and adjustment in the refining process can be promptly and accurately responded.
[0065]
Further, according to the present invention, the structure of the collected metal sample is refined by rapid solidification, so that there is no abnormal light emission during emission spectroscopic analysis, and the components of the metal sample can be analyzed with high accuracy. It is possible to accurately respond to component management and adjustment in the process.
[0066]
Furthermore, according to the present invention, two identical metal samples can be collected at the same time, so that one of them can be selected as an optimal analysis target sample, and one metal sample is used in terms of solidified structure. Even if defective, one of the metal samples can be used, so that the quickness of component management and adjustment in the refining process can be maintained.
[0067]
As described above, the present invention has a remarkable effect in controlling and adjusting components in the refining process. Therefore, the present invention has extremely high industrial value.
[Brief description of the drawings]
FIG. 1 is a diagram showing a cross section of a pump type sampler.
FIG. 2 is a diagram showing a cross section of a thick bottom type sampler provided with a quenching body.
FIG. 3 is a diagram showing one embodiment of a core part of the sampler for rapidly collecting metal samples according to the present invention.
FIG. 4 is a diagram showing an overall embodiment of a sampler for rapidly collecting metal samples according to the present invention.
FIG. 5 is a view showing another embodiment (two-cavity embodiment) of the core portion of the sampler for rapidly collecting metal samples according to the present invention.
FIG. 6 is a diagram showing the correspondence between the amounts of Ti in both samples collected by the method of the present invention and the conventional method.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 ... Container 2 ... Molten metal 3 ... Quenched body 4 ... Dish-shaped recess 5 ... Space partition plate 6 ... Spacer 7 ... Clip 8 ... Depression 9 ... Support rod 10 ... Ceramic lubricant 11 ... Metal sample 12 ... Metal sample rapid sampling sampler Core part 13 ... Fireproof ceramic cylinder 14 ... Slag mixing prevention paper cylinder 15 ... Holding support rod

Claims (10)

In a sampler that collects a metal sample from molten metal,
(A) providing at least one quenched body having at least one plane for rapidly solidifying a molten metal as a core part of a sampler;
(B) facing the plane, mounting a space partition plate made of a material that repels molten metal;
(C) The space between the plane and the space partition plate is a sample forming space in which the molten metal is rapidly solidified to form a metal sample.
A sampler for rapidly collecting metal samples. The sampler according to claim 1, wherein the quenching body is made of a material having a high heat removal capacity. 3. The metal sample according to claim 2, wherein the material having a high heat removal ability is a material composed of one or more of iron, steel, aluminum, copper, and stainless steel. 4. sampler. The sampler according to any one of claims 1 to 3, wherein the space partition plate is a plate made of a material having excellent thermal shock resistance and heat resistance and having a small amount of metal impurities. The sampler according to claim 4, wherein the plate made of a material having a small amount of metal impurities is a quartz glass plate. The sampler according to claim 1, wherein the thickness of the sample forming space is 0.5 to 20 mm. 7. The sampler according to claim 1, wherein the sample forming space has a gas vent hole. The metal sample rapid sampling sampler according to any one of claims 1 to 7, wherein a quenching body is combined so that the plane faces each other with a space partition plate interposed therebetween, thereby forming a core portion. In a sampling method of immersing a sampler in a molten metal and collecting a metal sample to be analyzed,
(A) immersing the metal sample rapid sampling sampler according to any one of claims 1 to 8 in a molten metal;
(B) quenching and solidifying the molten metal to form a metal sample in a sample forming space between the plane where the molten metal of the quenched body is rapidly solidified and the space dividing plate;
(C) peeling the space partition plate after pulling up the sampler and cooling,
A rapid sampling method characterized by the above-mentioned. In a sampling method of immersing a sampler in a molten metal and collecting a metal sample to be analyzed,
(A) immersing the metal sample rapid sampling sampler according to any one of claims 1 to 8 in a molten metal;
(B) quenching and solidifying the molten metal to form a metal sample in a sample forming space between the plane where the molten metal of the quenched body is rapidly solidified and the space dividing plate;
(C) After the sampler is pulled up and cooled, the space partition plate is peeled off,
(D) subjecting the metal sample to polishing and analysis while being welded to the flat surface of the quenched body,
A rapid sampling method characterized by the above-mentioned.

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